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Method for catalyzing, oxidizing and degrading 2-chloroethyl ethyl sulfide through multi-niobium-vanadium-oxygen clusters

A technology of chloroethyl ethyl sulfide and catalytic oxidation, which is applied in the field of catalytic chemistry, can solve the problems of uncontinuous use of catalyst, low conversion efficiency, low product selectivity, etc., and achieves low preparation cost, mild conditions, and easy acquisition. Effect

Inactive Publication Date: 2016-08-24
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned catalyst system has the problems of low conversion efficiency, low product selectivity, and continuous use of the catalyst, which makes it difficult for the current catalytic system to be practically applied.

Method used

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  • Method for catalyzing, oxidizing and degrading 2-chloroethyl ethyl sulfide through multi-niobium-vanadium-oxygen clusters
  • Method for catalyzing, oxidizing and degrading 2-chloroethyl ethyl sulfide through multi-niobium-vanadium-oxygen clusters
  • Method for catalyzing, oxidizing and degrading 2-chloroethyl ethyl sulfide through multi-niobium-vanadium-oxygen clusters

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Experimental program
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preparation example Construction

[0036] The preparation method of described hydrated niobium pentoxide is as follows:

[0037] Dissolve 1 g of niobium pentoxide in a mixed solution of 10 mL of nitric acid and hydrofluoric acid, add excess ammonia water, stir to obtain a precipitate of hydrated niobium pentoxide, wash the solid with deionized water until the pH value of the water is 7, and then Vacuum drying at 50°C to obtain hydrated niobium pentoxide; wherein the molar ratio of nitric acid and hydrofluoric acid is 1:3.

[0038] The K 7 Hb 6 o 19 13H 2 O was prepared as follows:

[0039] Mix 1g of niobium pentoxide with 1g of potassium hydroxide, bake in a muffle furnace at 1000°C for 24 hours, wash the obtained solid three times with 20ml of deionized water, and dry naturally to obtain K 7 Hb 6 o 19 13H 2 O.

Embodiment 1

[0041] A TMA 9 [PNb 12 o 40 (VO) 2 ] the method for catalytic oxidation degradation 2-chloroethyl ethyl sulfide, the method concrete steps are as follows:

[0042] (1) Take by weighing 100mg hydrated niobium pentoxide and 100mg vanadyl phosphate solid respectively and join in the polytetrafluoroethylene liner of stainless steel reactor, add 5g mass concentration and be the tetramethylammonium hydroxide aqueous solution of 25%, stir to make Mix well, adjust the pH value to 10 with phosphoric acid, and stir at room temperature for 1 hour. Seal the reaction kettle, put it in an oven, react at 160°C for 3 days, naturally cool to 20°C, filter the reaction solution, wash the filtrate with 20ml of isopropanol 3 times, and place it at room temperature for 2 days to evaporate the solvent and precipitate a solid. Filter, obtain light yellow solid after drying; Carry out XRD test to light yellow solid, test result is as follows figure 2 As shown, it can be seen that the result of t...

Embodiment 2

[0045] A TEA 9 [PNb 12 o 40 (VO) 2 ] the method for catalytic oxidation degradation 2-chloroethyl ethyl sulfide, the method concrete steps are as follows:

[0046] (1) Take by weighing 100mg niobium pentoxide hydrate and 100mg vanadyl phosphate solid respectively and join in the polytetrafluoroethylene liner of stainless steel reactor, add 5g mass concentration and be the tetraethylammonium hydroxide aqueous solution of 20%, stir to make Mix well, adjust the pH value to 11 with phosphoric acid, and stir at room temperature for 1 hour. Seal the reaction kettle, put it in an oven, react at 120°C for 4 days, cool naturally to 25°C, filter the reaction solution, wash the filtrate with 20ml of isopropanol 3 times, and place it at room temperature for 2 days to evaporate the solvent and precipitate a solid. Filter and dry to obtain a light yellow solid; carry out XRD test on the light yellow solid, it can be seen that the result of the light yellow solid is consistent with that ...

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Abstract

The invention discloses a method for catalyzing, oxidizing and degrading 2-chloroethyl ethyl sulfide through multi-niobium-vanadium-oxygen clusters and belongs to the field of catalytic chemistry. The method includes the steps that the 2-chloroethyl ethyl sulfide, a vanadium-cap type multi-niobium-vanadium-oxygen cluster catalyzing agent or a mixed multi-niobium-vanadium-oxygen cluster catalyzing agent and absolute methanol are added to a reaction vessel to be fully dissolved, a H2O2 aqueous solution is added dropwise, a reaction is conducted for a period of time under the stirring condition, and catalyzing, oxidizing and degrading of the 2-chloroethyl ethyl sulfide are completed. The conversion efficiency and product selectivity of the 2-chloroethyl ethyl sulfide are high, and the used multi-niobium-vanadium-oxygen cluster catalyzing agent can be used continuously; and furthermore, the conditions in the method are gentle, and the reaction can be conducted at the normal temperature under the normal pressure.

Description

technical field [0001] The invention relates to a method for catalytic oxidation degradation of 2-chloroethyl ethyl sulfide by using polyniobium vanadium clusters, in particular to a method for catalytic oxidation degradation of mustard gas analogue 2-chloroethyl ethyl sulfide by using multiple niobium vanadium clusters The method of ether belongs to the field of catalytic chemistry. Background technique [0002] Mustard gas is a typical chemical warfare agent, and its chemical composition is bis(2-chloroethyl)sulfide. It can cause strong irritation to human skin, eyes and respiratory tract, and can also damage the DNA structure of the human body, cause programmed cell death, and increase the risk of cancer. Therefore, the development of appropriate methods to rapidly and efficiently degrade mustard gas under mild conditions has received widespread attention. [0003] The degradation methods of mustard gas mainly include hydrolysis, elimination and partial oxidation. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A62D3/38B01J23/22A62D101/02A62D101/28
CPCA62D3/38A62D2101/02A62D2101/28B01J23/22
Inventor 胡长文迟瑛楠董婧胡菊芳
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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